Apparatus for producing carbon.



No. 872,950. PATENTED DEC. 3, 1907. J. MAOHTOLF. APPARATUS FOR PRODUCINGCARBON.

I APPLICATION FILED JULY2.1907. 2 SHEETS-SHEET 1.

PATBNTEU Uh}. 3, 1907.

APPLICATION FILED JULYZ. 1907.

2 SHEETS-SBEBT 2.

UNITED STATES PATENT oFFro JosErMAoH'roLr, or BoBLINcEN, GERMANY.

APPARATUS FOR PRODUCING CARBON.

Specification of Letters Patent.

Patented Dec. 3, 1907.

Original application filed llIarch 9. 1907, Serial No. 361.548. Dividedand this application filed 'Jul; 2; 1907- Serial No. 381,921.

T 0 all whom "it may concern:

Be it known that I, JosEF MACHTOLF, a subject of the King of Wurtemberg,residing at Boblingen, in the Kingdom of Wiirtemberg, Germany, haveinvented certain new and useful Improvements in Apparatus for ProducingCarbon; and I do hereby declare the following to be a full, clear, andexact description of the invention, such as will enable others skilledin the art to which it appertains to make and use the same.

This .invention relates to apparatus for producing carbon and consists uan apparatus adapted to produce a dissociative explosion in oil gas andother similar, normally inexplosive gases rich in carbon whereby a softlamp-black of desirable quality may be made; all as is more fullyhereinafter set forth and claimed.

In another application, Ser. No. 361548, filed March 9, 1907, I havedescribed and claimed a process of producing carbon blacks whichconsists essentially in producing a dissociative explosion of oil gasand similar carbon-rich gases of a normally inexplosive character; andthe present application relates to an apparatus particularly adapted tocarrying out the stated process.

In the prior art, lamp black has been produced by the explosion ofacetylene, but in practice it has been found that this black is too hardand granular, lacking the smooth, oil y glossiness which is desirable inpigment blacks. This low 'quality is largely due .to

the excessive high temperature produced in the explosion of acetylenewhich causes a molecular rearrangement of the carbon in harder form andalso causes destruction of the soft oily or tarry bodies which usuallyaccompany lamp black. .In the manufacture of printers ink this acetyleneblack is found to swell, which is a serious drawback,

and for lithography it isfound to lack gloss:

I have found that by heating to a suitable temperature, the normallyinexplosive hydrocarbon gases can also be caused to undergo adissociative explosion with the production of a carbon of much moredesirable quality. These carbonaceous gases, are all endothermic in theunion of hydrogen and carbon but not so highly so, as in the case ofacetylene, as to cause ready explosion. And,

being less endothermic their explosion must be facilitated by extraneousmeans and when produced does not yield, the high tem er ature of theacetylene explosion. T ese 'tion takes place.

means include preliminary heating, and, generally, some degree ofpressure. By suitable regulation of the initial heat and of the intialpressure, upon development of a dissociative explosion, carbons of themost varied characters can be produced, suited, for instance, for lndiaink, mk, printers ink, pencils, var- 'nish pigments, are carbons, etc.

As a suitable hydrocarbon, oil gas may be mentioned in the exam le ofthe process, but,

as already stated, any ydrocarbon, such for instance as coal gas, gasfrom raw naphtha and the like may be easily dissociated, that is reducedto carbon and hydrogen.

As above observed the oil gas or other hydrocarbon must be heatedprevious to the decomposition, that is to say, it must be brought to theproper temperature for division. This can take place in various ways. Inone arrangement the. heating is effected by aid of'the oil gas,acetylene, air or the like. In this manner the explosion chamber isadually heated so that when it'has reache the right temperature theaddition is -no longer necessary and gradually we can cease to makethese additions and work with pure oil gas. When this latter is the caseit suifices if there is added only a very small quantity of-acetylene,,-air or the like,

which merely sufiices' to commence the explosion.

According to another modification of the process the previous heating ofthe oil gas can be effected'by heating the apparatus with super-heatedsteam and at the same time regulating the initial pressure of the gas inthe apparatus so that the dissocia- In consequence of the heat liberatedby the ex losion the steam used for the heating wil be still furtherheated, which has the advantage that the initial ressure in the aparatus may be diminis ed, initial heat and initial pressure being tosome extent reciprocal.

After the explosion has taken place the carbon is collected in areceptacle from w 'ch it is filled into barrels.

he obtaining of the carbon is accompanied by the utilization of theliberated hydrogen, which latter can be drawn off from the of acetyleneand oil gas to explesion and the. I

heat thus liberated may be used for the heating of a Water jacketarranged around the ex sfloslon ap aratus.

ubstantia ly pure hydrogen is produced in the operation of the apparatusand this may be elsewhere utilized.

The above described process takes place with'entire exclusion of air,when in regular operation and is perfectly harmless and free from dustand smell, It should further be remarked that accordingto the presentprocess it is possible to not only produce enormous quantitiesofcarbonwith a small amount oflabor, but it is also possible to producethe carbon in' any desired condition; moreover, the roduction costs arefar smaller than hit erto. Exact calculations have shown that, the oilgas carbon is six times as cheap as acetylene carbon and is neverthelessbetter than the same. Exp'eriments which have been made by experts avefurther shown that a carbon which for instance has been produced from60% 'oil 'gas and 40% acetylene is specifically lighter than acetylenecarbon, its wei ht relative to the latter being in the ratio 0% about.968 to 1. The oil gas carbon is much more finely divided and thereforeis softer, wherefore it does not swell up when ground for the productionof printers ink, and'moreover it can be very easily mixed with water,which with acetylene carbon is not immediately the case. p j V In theaccompanying drawing is illustrated an a paratus by way of examplesuitable fort e carrying out of this process.-

In these drawings Figure l shows a view of the apparatus together withthe collector;

Fig. 2 is a longitudinal section thereof; Fig.

3 a view from above; 4 a horizontal section on the line A'A of Fig. 2;Fig. 5 a section through the gas inlet head, Fig. 6 a section throughthe stufiing box of the agitator; Fig. 7 a section through the lowerclosing valve of the dividing a paratus.

The apparatus consists oft e explosion cylinder 1 and the carboncollector 2 which stand in communication with one another by means ofthe tube 3. In the cylinder 1 the hydrocarbon gas is decomposed intocarbon and hydrogen and the carbon separating itself as lamp black isconveyed to the collector 2. The cylinder 1 formed of cast steel 1srovided asshown in Fi s. 2 and 4 with a ollow jacket 4, which 1sintended forthereception of the oil, water or steam used for thepreliminary heating. "For this purpose there is=placed at the upper partof the jacket 4 a projection 5 which acts either as a steam inlet or asoil outlet and the projection 6 at the lower art of the jacket servesin. like manner eit er let or an oil inlet. a

' At the top the cylinder is closed by means 6 5 ,of a cast steel. cover7 and underneath it is as a steam out-" .closed by a similar cast steelbottom 8. To the cover 7 there is attached the gas inlet head 9which asshown in Figs. 3 and 5 serves to carry on the one hand the ignitiondevice and on the other hand the gas inlet and outlet valves. The oilgas serving for the preparation of the lamp black is supplied throughthe projection 10, and through the projection 11 a priming gas(acetylene, air, or the like,) is introduced. Through the projection 12the hydrogen formed on the'decomposition is removed. The projections 10,11 and 12 are capable of being closed by the valves 22, 23 which can beeffected by means of the wheels 24,25. As these wheels are laced at aconsiderable height they arev pre erably connected .by means of thestrap .26 with an easily reached Wheel 27 (see Figs. 1 and 2).Theignition device consists of the ignition electrode13 placed in aprojection 14 provided witlrelectric lead 15, which electrode issurrounded by an insulating box 16; the whole having a constructionsimilar to that em loyed with gas engines.

n order to be able to cleanse the ignition device and the insulating boxwhen required, there is rovided in front thereof in the part 17, aspindle 19 placed in the front part 18. This spindle 19 stands under thepressure of a spring 20 and is operated by means of a wheel 21. Thewheel 21 can be connected .by means of a strap with a-second wheel sothat the cleansing can take place from any point. I

The spindle 19 has two purposes; on the one hand, in starting theapparatus, by pressing it in and then releasing it, the first spark orthe first explosion is obtained. This manipulation is necessary severaltimes until short-circuit and the spark is produced as soon as thecurrent circuit is closed. In this manner there is formed a veritablespark producer. On the other hand the spindle, as already stated, servesfor cleaning the insulating box, if it should happen that too much lampblack is collected in this apparatus, in'which case the current wouldpass over without sparking. This accident, however, can very rarelyhappen because in the inrush of the gases the lamp black is alwayscarried forward with them. i

The gas head 9 is further provided with a pressure gage 42 in order toindicate the gas pressure at all times. On the project1on28 of the base8 there is a closing valve 30'pr0- vided with a wheel 29 which valve hasfor its purpose to interrupt the-connection with the collector 2during'the decomposition of the hydrocarbon gas. In Fig. 7, this lowerpart isillustrated on a larger scale.

Within he cylinder 1 there is placed astuffing box 52 secured a strap37. Upon the hollow axle 34 there is a revoluble valve body 38 (Fig. 2)which possesses a spring back pressure valve 39 and a projection 40,which serves for the introduction of hydrogen and can be placed incommunication with the same hydrogen container as the outlet piece 12.

In order to insure that the valve 39 is closed before the explosion ofthe hydrocarbon gas begins, it is advisable to provide the back pressurevalve 39 with a lever (not shown) for the'motion thereof, so thathydrogen passing through the part 40 may not be opposed by the spring41. The back pressure valve 39 is formed as a conical valve on which theelement 40 can rotatably move.

In the collector there is, as stated, the lamp black gathered from thecylinder 1. In order to facilitate the removal of this black it isadvisable to make .use of the apparatus shown in Fi s. 1 and 2. Beneaththe prolongation 43 of the container 2 is provided asoot catcher 45, atight joint being made between the two by rubber gasket 44. A threaded sindle 48, seated in 46, and provided with p ate 47 can be operated topress the soot catcher upwards against the gasket and element 43.

Compression of the lamp black into the barrel 45 takes place by means ofa piston 49, the rod 50 whereof passes through a above to the cover 51of thereceptacle 2. The'actuation of the piston may be performed bymeans of a suitable transmission device from any convenient point. Tothe cover 51 of the receptacle 2 there is attached a tube 53 whichstands in connection with a dust collecting device not shown in thedrawing. The. operation of the apparatus described is as follows:

When using oil gas with acetylene or the like, and starting theapparatus the hollow jacket 4 is filled with gas oil and the tube 5brought into connection with the oil gas producer (not shown) so thatthe previously heated oil can flow through the projection 5 while thereis introduced through the projection 6 enough cold oil to insure thatthe cylinder 1 always maintains the desired temperature. Before,however, the first explosion is brought about oil gas is admittedthrough the projection, 10 into the apparatus until all the air isdriven out. In subsequent operation, the hydrogen remaining in thecylinder may be similarly displaced. Any hydrogen not displaced andremaining in the oil gas does no harm. closed and through the projection11 acetylene'gas under a pressure of about four atmospheres isintroduced into the cylinder. Then the valve 22 connected to the gashead is closed and the mixture of gas which is now in the cylinder 1 ismade to explode by means of the ignition device 13, whereupon themixture of oil gas and acetylene is decomposed into carbon and hydrogen.The valve 23 is then opened and the liberated hydrogen is drawn off intoa gas holder (not shown) through the connection 12. This gas holder iscomposed of a closed vessel which may suitably have the same capacity asthe cylinder so that in the cylinder and in the hydrogen holder the samepressure prevails. The hydrogen valve 23 is then closed and the stirrers3 1, 32 of the collecting vessel 2 are set in motion. While the stirrersare in operation the valve 30 is opened, whereby the hydrogen stillremaining in the cylinder 1 drives the carbon, that is to say, the lampblack into the collector 2. As soon as the pressure in the cylinder '1disappears the back pressure valve 39 opens and hydrogen flows inwardthrough the projection 40 and The valve 30is then hollow axle 34 intothe steel tube 32 of the stirrer and outward through its perforations,whereby any carbon still remaining on the inner wall of the cylinder 1is entirely blown away. Whatever therefore, has not been scraped off bythe knife 31 is entirely re moved by means of the hydrogen flowingthrough the tube 32. After the carbon has been thoroughly removed fromthe cylinder 1, in this manner the agitator is stopped, the valve 30 isclosed, and by opening the valve 23 the cylinder is again filled withgas for the purpose of anotherexplosion. Through the heat caused by thesuccessive explosions the cylinder becomes more and more heated. With aprevious warming to 300 centigrade a mixture of 90% oil gas with 10%acetylene suffices in order to bring'about the reaction. With atemperature of 350 to 380 centigrade in the container, traces ofacetylene are necessary to cause the explosion of oil gas. When theapparatus is full of oil gas under the' desired pressure, which may betwo or three atmospheres, about one-fifth of a liter of acetylene gas ispumped in through 1 1 into the head 9 by means ofa hand pump. In thismanner there is provided in the hollow space of the head 9 an easilyexplosible mixture which suffices to bring about the reaction.

In place of the acetylene another explodible priming gas may be used inthe same manner. As has been shown by experiment a few cubic centimetersof air may be pumped in without danger. The pressure and the temperaturemust of course always which is being used, and in the case of a gasricher in carbon it is possible to operate at' the collector 2 is takenthrough the tube 53 into a receptacle (not shown) which serves as asootcollector, small quantities of lamp black being carried along by thehydrogen.

In order to utilize the process for oil gas without using acetylene orthe like superheated steam is introduced through the projeotion 5 andthe cylinder is heated in this manner. The cooled steam or the condensedwater is drawn off through the port 6. After the apparatus is heated upto about 150 centigrade if there be used a gas which does not decomposeat this temperature un der a pressure of about five atmospheres, thenthe. pressure must be so far increased that the decomposition can takeplace. 'The heat liberated by the explosion will soon bring theapparatus to a temperature at wiii'ch working under lower pressure isposs1 e. such as acetylene or a little air admixed with the gas in thehead of the cylinder may also be here used in starting.

' When the collector 2 is filled with carbon, which of course onlyoccurs after a whole series of explosions, the carbon is fiflled intodelivery cask 45 in .the manner-already set forth. In this connection itmust be further observed that the motion of the'aforesaid pressurepiston 49 can be effected either by and or by machinery. When the pistonis in its lowermost ositionit closes the collector 2 tightly so t at nohydrogen can escape. The upward access of air in any material amountinto the collectorwill not occur be "cause 111 consequence of thedifference of specific gravity between air and hydrogen though hydrogenwill escape downward no air can enter the collector during the brieftime the apparatus is open.

By means of a corresponding device it is even possible to fill the caskswith hydrogen or to drive out the air from them before the iston 49 israised. For this purpose it sufces to make a little hole at the top andsidewise underneath in the cask 45 and to bring these holes intoconnection with hydrogen supply pipe so that the 'air is driven out ofthe casks from above downwards. This is,

However, an explosive priming gas,

Moreover, it s veryor in the collector 2 will take place, because thelamp black is never delivered to it at such a temperature that it canignite as has been ex erimentally proved. The expansion of t e ases inemptying the cylinder cools down tIie carbon.

In using a plurality of explosion cylinders, it is not necessary toemploy a special steam generator to furnish steam for heating thejackets since one such device may be em' ployed to furnish steam for theothers. For instance one such device may have its jacket supplied withwater and be used to explode a mixture of per cent. acetyleneand 20 percent. oil gas. The heat developed from such a mixture will furnishplenty of steam. It is also possible to use another such device tosuperheat the steam furnished by the first. By heat-insulating the steamconduits in the usual way, dry hot steam may be delivered from one suchdevice, functioning as a steam generator into the jackets of the otherdevices.

In the normal operation of the apparatus here shown an excess of heat isgenerated and this may be employed in any suitable manner. The largequantity of hydrogen produced may also be employed in any suitablemanner, as, for instance, in heatingoil gas retorts supplying oil gas tothe apparatus, for formin ammonia with nitrogen, in motors, or fororming acetylene by uniting it with carbon. i

The attention to the whole apparatus can be efiected from any point. It1s therefore i not necessary'that the workmen are laced in the same roomas the apparatus. he arran ement can also be constructe d so as to worcontinuously and automatically without the necessity for manualoperation of I valves and the like, by the use of suitable gearing andother mechanism. 7

' Having thus fully described my invention, what I claim as new, is 1 1.In an apparatus for the production of amorphous carbon, the combination,with a decomposition chamber provided with controllable means forproducing explosive decomposition therein, of a collection chamber, aconduit connectin the decomposition 1 chamber with the col ectionchamber, and means for controlling the conduit.

-2. In an apparatus for the production of amorphous carbon, thecombination, with a decomposition chamber, means for supplying 1 anexplosive fluid thereto,.and controllable means for igniting said fluidexplosively, of a collection chamber, and means for putting thecollection chamber and the decom osition chamber in connection with eachot er. 1 3. In an apparatus for the production of amorphous carbon, thecombination, with a decomposition cylinder, means for supplying anexplosive hydrocarbon mixture to the same, and means for igniting'saidmixture 1 explosively, of means for removing soot from mechanism havinga-hollow axis, a valve said explosion chamber, and'a scraper mechbod;with which said axis communicates, 35 anism within the decompositionchamber. means for supplying a fluid to said valve 4. In an apparatusfor the production of body, and a valve in the valve body. amorphouscarbon, the combination, with a 8. Inan ap' aratus for producing amor-'decomposition chamber provided with conphous carbon, the combination,with 'a detroll'able means for producing explosive decompositiontherein, of a collection chamber connected therewith, and means forremoving soot from thecollection chamber.

5. In an apparatus for producing amorphous carbon, the combination, witha decomposition chamber provided with controllable means for producingexplosive decomposition therein, and a collection chamber connectedthereto, of means for attaching .a receptacle to the collection chamber,and means for discharging the contents of the collection chamber intothe receptacle.

20. 6. In an apparatusfor producing amorphous carbon, the combination,with a decomposition chamber provided with control lable means forproducing explosive decomposition therein, of a scraping mechanismtrollable means for producing explosive decomposition therein, and acollection 'cham- .ber valve connected therewith, of a compacting anddischarging piston movable in said collection chamber, and means-formoving said piston to discharge the contents of the collection chamber.n

9. In an apparatus for producing amorphous carbon, the combination, witha decomposition chamber, provided with controllable means for producingexplosive decomposition therein, and having in open butclosableconnection therewitha collection chamber having a cover, of a piston inthe collection chamber, a piston rod connected to the piston, a packinggland on the cover of the collection chamber, through which the 25arranged to scrape the interior walls of the piston rod passes, and aconnection between decomposition chamber, said scraping mechthedecomposition chamber and the collec- -anism comprising a perforatedtube arranged tion chamber.

to discharge a fluid against said walls. In testimony whereof I hereuntoaffix my 7. In an apparatus for producin amorsignature in thepresencgaof two witnesses.

' J OS F 30 phous carbon, the combinat1on,vv1t a de- MACI-ITOLF.

composition chamber provided with con- Witnesses: I trollable means forproducing explosive de- AnoLF Lnnnnns,

composition therein, of a rotatable scraping Ennns'r .ENrnnMAnN.

composition chamber provided with con-'40

